HRID990843
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a solution of (3,5-dichloro-4-hydroxy-phenyl)-carbamic acid tert-butyl ester (1.0 g) and potassium carbonate (1.0 g) in acetone (18 mL) is added ethyl iodide (0.36 mL) and the mixture is stirred for approximately 15 hours at room temperature. The solution is then filtered, concentrated under reduced pressure, and partitioned between ethyl acetate and water. The separated aqueous layer is further extracted twice with ethyl acetate, and the pooled organic extracts are washed successively with 10% aqueous sodium hydroxide, with water, and then dried over anhydrous sodium sulfate. Evaporation of the solvent under reduced pressure gave the desired product as a tan solid.
WORKUP
后处理
- filtrationThe solution is then filtered
- concentrationconcentrated under reduced pressure
- custompartitioned between ethyl acetate and water
- extractionThe separated aqueous layer is further extracted twice with ethyl acetate
- washthe pooled organic extracts are washed successively with 10% aqueous sodium hydroxide, with water
- dry with materialdried over anhydrous sodium sulfate
- customEvaporation of the solvent under reduced pressure